CN105170158A - CoMn composite oxide catalyst for eliminating benzene-serial volatile organic compounds in air and preparation method for therefor - Google Patents
CoMn composite oxide catalyst for eliminating benzene-serial volatile organic compounds in air and preparation method for therefor Download PDFInfo
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Abstract
The invention discloses a CoMn composite oxide catalyst for eliminating benzene-serial volatile organic compounds in air and a preparation method for therefor. The active component of the catalyst is CoMn spinel oxide. The catalyst disclosed by the invention has the advantages that by using the spinel composite oxide formed by non-noble metals Co and Mn as the active component, the cost of the catalyst is lowered to a great extent; a spinel phase of the catalyst provides an active specie MnCo2O4 for catalytic combustion reaction for benzene-serial volatile organic compound reactant molecules, so that the catalyst has good catalytic combustion activity for low-temperature benzene-serial volatile organic compound. According to the catalyst disclosed by the invention, Co and Mn salt is used for preparing the CoMn composite oxide catalyst by taking spinel as the main active component by virtue of complexometry. The method is simple in process, mild and easily controllable in condition and good in repeatability.
Description
Technical field
The present invention relates to a kind of benzene series volatile organic compounds by catalytic combustion catalyst, be specifically related to a kind ofly eliminate CoMn composite oxide catalysts of benzene in air system volatile organic matter and preparation method thereof.
Background technology
In today that environment for human survival goes from bad to worse, environmental pollution receives great attention, and atmospheric environment is as one of important living environment of the mankind, and its pollution situation is paid much attention to equally.Volatile organic matter (VolatileOrganicCompounds, VOCs) be the important component part of atmosphere pollution, VOCs is of a great variety, complicated component, great harm is had to health and environment, in these VOCs, the harm of benzene series volatile organic matter (e.g., benzene,toluene,xylene etc.) is more outstanding.Benzene series volatile organic matter is mainly derived from petrochemical industry waste gas, is iron and steel manufacture, semiconductor components and devices production, petrochemical industry, pharmacy, printing, shoemaking, sprays paint etc. that industry is modal to discharge pollutants.Because benzene series volatile organic matter has volatile feature, the multiplex toluene of house decorative material, dimethylbenzene replace purified petroleum benzin as the solvent of the materials such as various glue, paint, coating or diluent, and therefore, interior decoration is also important benzo pollutants source.Benzene series volatile organic matter has mutagenesis, teratogenesis and carcinogenic " three cause " harm to human body, and caused the great attention of countries in the world, WHO is defined as strong carcinogen benzene series volatile organic matter.World many countries has formulated the atomosphere quality standard of benzene series volatile organic matter, is 5 μ g/m as European Union performed the average annual concentration limit of benzene in air from 1 day December in 2000
3, rising on January 1st, 2006 is 1 μ g/m
3.In the World Health Organization (WHO) regulation air, the per day exposure concentration limit value of toluene is 8.21 μ g/m
3.Benzene series volatile organic matter also has close ties with Atmospheric Photochemical Smog, aerocolloidal formation, can generate the photochemical fog that toxicity is larger.
Processing method for benzene series volatile organic matter can be divided into two large classes usually: a class is non-destructive technique and absorption method; One class is destructive technology, namely make benzene series volatile organic matter be converted into the inorganic matter that carbon dioxide, water and hydrogen chloride etc. are nontoxic or toxicity is little by chemistry or biological technology, these class methods comprise the common technique such as direct burning, catalytic combustion, biodegradation, plasma oxidation, photocatalytic oxidation.Wherein, catalytic combustion can process the benzene series volatile organic matter gas of low concentration under far below direct ignition temperature (>500 DEG C) condition, having the advantages that purification efficiency is high, non-secondary pollution, energy consumption are low, is one of the most effective processing method of process benzene series volatile organic matter application.Domestic and international researcher has carried out a large amount of correlative study to catalyst for catalytic combustion, and the purification treatment technology of benzene series volatile organic matter has become a study hotspot in environmental catalysis field in air, and the key problem of correlative study is still the problem of the design and development of catalysis material.At present, benzene series volatile organic compounds by catalytic combustion catalyst used mainly contains noble metal catalyst, comprises containing Pt, Pd, Ru and Au etc., due to high, selective good, the long service life of its activity, and there is the advantages such as good antitoxin performance, cause the great interest of researcher.Although noble metal catalyst has lot of advantages, due to its expensive and limit noble metal catalyst benzene series volatile organic matter eliminate in application.Therefore, cheap in recent years catalyst of transition metal oxide causes the broad interest of people.Research for catalyst of transition metal oxide finds, mixed oxide catalyst shows superior catalytic activity and stability, even can reach the catalytic effect of noble metal catalyst, and price exist very large advantage, and easily obtain, therefore have broad application prospects.
Transition metal oxide is subject to each field extensive concern as the functional material that a class is important, at catalytic field, composite oxide material is used as catalyst, has higher catalytic performance than single component catalyst.But there is the defects such as active component content is low, compact structure in the metal oxide that conventional method obtains, this significantly limits the performance of its catalytic performance.Therefore, adopting suitable method to obtain and have high activated catalyst, is also one of research work center of gravity of researchers.Carry out the research of composite oxide catalysts preparation and benzene series volatile organic matter catalytic removal performance; not only to the Synthesis and applications of oxide, there is important using value and scientific meaning, the catalytic removal of benzene series volatile organic matter and atmospheric environment protection are also had great importance.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of CoMn composite oxide catalysts eliminating benzene in air system volatile organic matter, this catalyst is with low cost and to have good low temperature benzene series volatile organic compounds by catalytic combustion active; Present invention also offers the preparation method of above-mentioned catalyst.
The technical scheme that the present invention takes is as follows:
Eliminate the CoMn composite oxide catalysts of benzene in air system volatile organic matter, the active component of described catalyst is CoMn spinel oxide.
The preparation method of above-mentioned catalyst, comprises the following steps:
1) by complexing agent: the molar ratio of cobalt salt, manganese salt sum=1 ~ 1.8:1, is mixed with solution by three, then evaporate to dryness obtains siccative;
2) by step 1) siccative that obtains carries out roasting, and roasting condition is be warming up to 300 ~ 450 DEG C with the heating rate of 10 DEG C/min, then constant temperature calcining 2.0 ~ 4.0h and get final product at 300 ~ 450 DEG C.
Preferably, described step 1) described in complexing agent be citric acid.
Preferably, described step 1) described in mol ratio between cobalt salt and manganese salt be 2 ~ 6:1.
Preferred, described step 1) described in mol ratio between cobalt salt and manganese salt be 4:1.
Preferred, described step 1) middle ratio, described complexing agent: cobalt salt, manganese salt sum=1.5:1.
Preferably, described step 1) described in cobalt salt be cobalt nitrate, described manganese salt is manganese nitrate.
Preferably, described step 1) described in evaporate to dryness condition be at 80 ~ 100 DEG C, continue dry 12 ~ 24h after 80 DEG C of evaporates to dryness.
Preferably, described step 2) in roasting condition be roasting 3h at 350 DEG C.
Beneficial effect of the present invention is:
1) with base metal Co and Mn formed spinel complex oxide for active component, considerably reduce catalyst cost;
2) the spinelle thing phase (MnCo of CoMn composite oxide catalysts of the present invention
2o
4), for the catalyst combustion reaction of benzene series volatile organic matter reactant molecule provides active specy, therefore, CoMn composite oxide catalysts of the present invention is at high reaction velocity (66,000mLh
-1g
-1), to show good benzene series volatile organic compounds by catalytic combustion under low reaction temperature (<180 DEG C) active, has good low temperature benzene series volatile organic compounds by catalytic combustion active;
3) Co and Mn salt is obtained by complexometry with spinelle by the present invention is the CoMn composite oxide catalysts of main active component, and the method technique is simple, and mild condition is easily controlled, reproducible.
Accompanying drawing explanation
In order to make object of the present invention, technical scheme and beneficial effect clearly, the invention provides following accompanying drawing:
CoMn composite oxide catalysts XRD spectra obtained under the different sintering temperature of Fig. 1;
H under the different sintering temperature of Fig. 2
2temperature programmed reduction curve;
The CoMn composite oxide catalysts XRD spectra that different CA/ (Co+Mn) mol ratio of Fig. 3 is obtained;
The CoMn composite oxide catalysts XRD spectra that the different Co/Mn mol ratio of Fig. 4 is obtained.
Detailed description of the invention
Below the preferred embodiments of the present invention are described in detail.The experimental technique of unreceipted actual conditions in embodiment, the usually conveniently conditioned disjunction condition of advising according to manufacturer.
Eliminate the CoMn composite oxide catalysts of benzene in air system volatile organic matter, the active component of described catalyst is CoMn spinel oxide, and the preparation method of described catalyst comprises the following steps:
(1) by citric acid: the molar ratio of (cobalt nitrate and manganese nitrate sum)=1 ~ 1.8:1, is mixed with solution by three, solution is continued after 80 DEG C of evaporates to dryness at 80 ~ 100 DEG C dry 12 ~ 24h and obtain siccative; Mol ratio between cobalt nitrate and manganese nitrate is 2 ~ 6:1;
(2) by step 1) siccative that obtains carries out roasting, and roasting condition is be warming up to 300 ~ 450 DEG C with the heating rate of 10 DEG C/min, then constant temperature calcining 2.0 ~ 4.0h and get final product at 300 ~ 450 DEG C.
Embodiment 1 sintering temperature is on the impact of catalyst performance
Be 4:1 by the mol ratio (Co/Mn) between cobalt nitrate and manganese nitrate, citric acid: the mol ratio (CA/M of (Co+Mn), M=Co+Mn) be 1.5:1, sintering temperature is 300,350,400,450 DEG C, roasting time 3h, preparation CoMn composite oxide catalysts, is used for toluene catalytic combustion by catalyst, carries out the activity rating of catalyst; The activity rating of catalyst is carry out in the miniature tubular fixed-bed reactor of 8mm at ambient pressure in internal diameter, and thermocouple is built in reactor, reaction temperature by
type temperature programming controller controls, and microreactor is placed in tube furnace; Toluene waste gas by volume percentage comprises: toluene 1.0% and air 99.0%; Concrete operation step is as follows:
Measure 50mg catalyst to load in the reaction tube of miniature tubular fixed-bed reactor, be warmed up to reaction temperature, pass into the toluene waste gas of described composition, at this reaction temperature and 66,000mLh
-1g
-1under reaction gas space velocities, constant temperature eliminates toluene (air mass flow is controlled by flowmeter), by residual toluene content in the GC-7900II type gas-chromatography on-line checkingi tail gas of band hydrogen flame detector, testing conditions is: detector temperature 120 DEG C, injector temperature 433K, post case temperature perseverance is 433K.
The benzene series volatile organic compounds by catalytic combustion conversion results of the CoMn composite oxide catalysts that above-mentioned catalyst activity evaluation experimental obtains is as shown in table 1:
Table 1 sintering temperature is on the impact of catalyst toluene catalytic combustion performance
As shown in Table 1, when temperature is 350 DEG C, toluene conversion effect is best, and when reaction temperature is 180 DEG C, toluene conversion can reach 99.9%.
CoMn composite oxide catalysts XRD spectra obtained under different sintering temperature as shown in Figure 1, from XRD spectra, obtained CoMn oxide catalyst is all based on CoMn spinel oxide, along with the increase of sintering temperature, the crystalline phase of catalyst does not change, but its degree of crystallinity increases to some extent.
H as shown in Figure 2
2temperature programmed reduction curve is known, and the CoMn composite oxide catalysts obtained by citric acid complex method has the reducible performance of high low temperature.Show thus, obtained CoMn composite oxide catalysts for toluene catalytic combustion reaction provides active oxygen species under low reaction temperature, thus can promote the low-temperature catalytic burning of toluene.Low sintering temperature is unfavorable for the activation to catalyst, and shows the reducible performance of low temperature of going on business; High sintering temperature can cause catalyst excess agglomeration and reduce reducible performance, capital causes the reducible performance of the low temperature of corresponding catalyst to reduce, namely the ability that low temperature produces active oxygen species reduces, thus the toluene catalytic combustion causing catalyst show going on business activity.Therefore, the sintering temperature (the present invention is 350 DEG C) of adaptation is necessary for preparation CoMn composite oxide catalysts.
Embodiment 2 citric acid: the mol ratio (CA/M, M=Co+Mn) of (Co+Mn) is on the impact of catalyst performance
Mol ratio (Co/Mn) between cobalt nitrate and manganese nitrate is 4:1, sintering temperature is 350 DEG C, roasting time is under 3.0h condition, different citric acids is set: the mol ratio of (Co+Mn), preparation CoMn composite oxide catalysts, catalyst is used for toluene catalytic combustion, carries out the activity rating of catalyst, activity rating method is with embodiment 1.
The benzene series volatile organic compounds by catalytic combustion conversion results of the CoMn composite oxide catalysts that above-mentioned catalyst activity evaluation experimental obtains is as shown in table 2:
Table 2 citric acid: mol ratio (CA/M (the M=Co+Mn)) impact on toluene catalytic combustion performance of (Co+Mn)
As shown in Table 2, when the mol ratio of citric acid and cobalt nitrate and manganese nitrate sum is 1.5:1, toluene conversion effect is best, and when reaction temperature is 180 DEG C, toluene conversion can reach 99.9%.
The CoMn composite oxide catalysts XRD spectra that different CA/M mol ratio obtains as shown in Figure 3, from XRD spectra, obtained CoMn oxide catalyst all based on CoMn spinel oxide, along with the crystalline phase of the change catalyst of CA/M mol ratio does not change.
Embodiment 3Co/Mn mol ratio is on the impact of catalyst combustibility
At citric acid: the mol ratio of (Co+Mn) is 1.5:1, sintering temperature is 350 DEG C, roasting time is under 3.0h condition, mol ratio between different cobalt nitrates and manganese nitrate is set, preparation CoMn composite oxide catalysts, catalyst is used for toluene catalytic combustion, carries out the activity rating of catalyst, activity rating method is with embodiment 1.
The benzene series volatile organic compounds by catalytic combustion conversion results of the CoMn composite oxide catalysts that above-mentioned catalyst activity evaluation experimental obtains is as shown in table 3:
Table 3Co/Mn mol ratio is on the impact of toluene catalytic combustion performance
As shown in Table 3, when Co/Mn mol ratio is 4:1, toluene conversion effect is best, and when reaction temperature is 180 DEG C, toluene conversion can reach 99.9%.
The CoMn composite oxide catalysts XRD spectra that different Co/Mn mol ratio obtains as shown in Figure 4, from XRD spectra, CoMn oxide catalyst obtained by different Co/Mn mol ratio is all based on CoMn spinel oxide, along with the increase of Co/Mn mol ratio, the crystalline phase of catalyst does not change, but its degree of crystallinity increases to some extent.
The CoMn composite oxide catalysts that embodiment 4 optimum condition obtains is on the impact of benzene homologues catalytic combustion properties
Be 1.5:1 in CA/ (Co+Mn) mol ratio, Co/Mn mol ratio is 4:1, sintering temperature is 350 DEG C, roasting time is under 3h condition, preparation CoMn composite oxide catalysts, catalyst is used for benzene homologues catalytic combustion, carries out the activity rating of catalyst, activity rating method is with embodiment 1.
The benzene series volatile organic compounds by catalytic combustion conversion results of the CoMn composite oxide catalysts that above-mentioned catalyst activity evaluation experimental obtains is as shown in table 4:
The catalytic combustion result of table 4 benzene series volatile organic matter
As shown in Table 4, CoMn composite oxide catalysts all has good catalytic combustion activity to benzene, toluene, ethylbenzene and dimethylbenzene, and especially to toluene, ethylbenzene and dimethylbenzene, not higher than under the reaction temperature of 220 DEG C, the conversion ratio of three is all more than 90%.
What finally illustrate is, above preferred embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by above preferred embodiment to invention has been detailed description, but those skilled in the art are to be understood that, various change can be made to it in the form and details, and not depart from claims of the present invention limited range.
Claims (9)
1. eliminate the CoMn composite oxide catalysts of benzene in air system volatile organic matter, it is characterized in that, the active component of described catalyst is CoMn spinel oxide.
2. the preparation method of CoMn composite oxide catalysts described in claim 1, is characterized in that, comprise the following steps:
1) by complexing agent: the molar ratio of cobalt salt, manganese salt sum=1 ~ 1.8:1, is mixed with solution by three, then evaporate to dryness obtains siccative;
2) by step 1) siccative that obtains carries out roasting, and roasting condition is be warming up to 300 ~ 450 DEG C with the heating rate of 10 DEG C/min, then constant temperature calcining 2.0 ~ 4.0h and get final product at 300 ~ 450 DEG C.
3. the preparation method of CoMn composite oxide catalysts according to claim 2, is characterized in that, described step 1) described in complexing agent be citric acid.
4. the preparation method of CoMn composite oxide catalysts according to claim 2, is characterized in that, described step 1) described in mol ratio between cobalt salt and manganese salt be 2 ~ 6:1.
5. the preparation method of CoMn composite oxide catalysts according to claim 2, is characterized in that, described step 1) described in mol ratio between cobalt salt and manganese salt be 4:1.
6. the preparation method of CoMn composite oxide catalysts according to claim 2, is characterized in that, described step 1) middle ratio, described complexing agent: cobalt salt, manganese salt sum=1.5:1.
7. the preparation method of CoMn composite oxide catalysts according to claim 2, is characterized in that, described step 1) described in cobalt salt be cobalt nitrate, described manganese salt is manganese nitrate.
8. the preparation method of CoMn composite oxide catalysts according to claim 2, is characterized in that, described step 1) described in evaporate to dryness condition be at 80 ~ 100 DEG C, continue dry 12 ~ 24h after 80 DEG C of evaporates to dryness.
9. the preparation method of CoMn composite oxide catalysts according to claim 2, is characterized in that, described step 2) in roasting condition be roasting 3h at 350 DEG C.
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|---|---|---|---|---|
| CN106622212A (en) * | 2016-12-08 | 2017-05-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Manganese-based catalyst for volatile organic compound governance, and preparation and application thereof |
| CN106693985A (en) * | 2016-11-24 | 2017-05-24 | 上海交通大学 | Preparation method of sheet spinel structure cobalt-manganese composite oxide |
| CN108525674A (en) * | 2018-03-27 | 2018-09-14 | 上海倍绿环保科技有限公司 | Couple the cobalt manganese O composite metallic oxide catalyst and preparation method thereof of electrostatic field collaboration removal low-concentration methane gas |
| CN108682869A (en) * | 2018-04-10 | 2018-10-19 | 云南铝业股份有限公司 | Manganese cobalt spinel oxygen reduction catalyst and preparation method thereof |
| CN109319912A (en) * | 2018-09-18 | 2019-02-12 | 重庆工商大学 | A method of quinoline waste water is handled using CeCu oxide catalyst |
| CN110193368A (en) * | 2019-06-21 | 2019-09-03 | 河北科技大学 | A kind of preparation method of spinel-type catalysis material |
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| CN110844944A (en) * | 2019-11-29 | 2020-02-28 | 昆明理工大学 | Preparation method of Ce-Mn-Co-O oxygen carrier and application of Ce-Mn-Co-O oxygen carrier in chemical looping reforming hydrogen production of blast furnace gas |
| CN110975870A (en) * | 2019-12-12 | 2020-04-10 | 重庆工商大学 | Preparation method and application of copper-cobalt composite oxide catalyst |
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| CN106622212B (en) * | 2016-12-08 | 2019-06-21 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of manganese-based catalyst administered for volatile organic matter and preparation and application |
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| CN113617373B (en) * | 2021-08-06 | 2023-07-25 | 大连海事大学 | Catalyst for removing volatile organic compounds and preparation method thereof |
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